Method for determining residual quantity of glyphosate, glufosinate-ammonium and metabolite aminomethylphosphonic acid of glyphosate and glufosinate-ammonium in agricultural products

A technology of aminomethylphosphonic acid and medium glyphosate, which is applied in chemical instruments and methods, measuring devices, and other chemical processes, can solve the problems of reproducibility and poor precision of analysis results, and achieve short time-consuming, High detection efficiency and accurate quantitative results

Pending Publication Date: 2022-04-12
WUHAN ACADEMY OF AGRI SCI
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  • Abstract
  • Description
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Problems solved by technology

Analytical methods such as high-performance liquid chromatography have high requirements for pre-treatment. When analyzing complex organic matter, the reproducibility and precision of the ana

Method used

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  • Method for determining residual quantity of glyphosate, glufosinate-ammonium and metabolite aminomethylphosphonic acid of glyphosate and glufosinate-ammonium in agricultural products
  • Method for determining residual quantity of glyphosate, glufosinate-ammonium and metabolite aminomethylphosphonic acid of glyphosate and glufosinate-ammonium in agricultural products
  • Method for determining residual quantity of glyphosate, glufosinate-ammonium and metabolite aminomethylphosphonic acid of glyphosate and glufosinate-ammonium in agricultural products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Determination of glyphosate, glufosinate-ammonium and aminomethylphosphonic acid residues in rice samples.

[0046] (1) Sample pretreatment

[0047] Weigh 2g of rice sample into a 50mL EP tube, pulverize it thoroughly, then add 10mL of deionized water and 10mL of dichloromethane in turn, mix and shake for 60min, then centrifuge at 8000r / min for 10min, take 5mL of the supernatant; 10mL of methanol and 10mL of water were used to activate the C18 solid-phase microextraction column. After the activation was completed, let it stand for 5 minutes; take the above-mentioned clear liquid onto the column for purification treatment. It is worth noting that the flow rate of the clear liquid through the SPE column should not exceed 6 μL / s , collect the effluent; finally, the purified sample is detected by liquid chromatography-mass spectrometry.

[0048] (2) Preparation of standard working solution:

[0049] Use the rice that has been tested to be free of glyphosate, glufosinate a...

Embodiment 2

[0104] Determination of glyphosate, glufosinate-ammonium and aminomethylphosphonic acid residues in lettuce samples.

[0105] (1) Sample pretreatment

[0106] Weigh 5g lettuce sample in a 50mL EP tube, pulverize it thoroughly, then add 10mL deionized water and 10mL dichloromethane in turn, mix and shake for 60min, then centrifuge at 8000r / min for 10min, take 9mL supernatant, and then Add 1mL of acetonitrile; use 10mL of methanol and 10mL of water to activate the C18 solid-phase microextraction column successively, and let it stand for 5 minutes after the activation; take the above-mentioned clear liquid onto the column for purification treatment. It is worth noting that the flow rate cannot be faster than 6μL / s, the effluent was collected; finally, the purified sample was detected by liquid chromatography-mass spectrometry.

[0107] (2) Preparation of standard working solution

[0108] Use the lettuce that has been tested to be free of glyphosate, glufosinate and aminomethy...

Embodiment 3

[0117] Determination of glyphosate, glufosinate-ammonium and aminomethylphosphonic acid residues in potato samples.

[0118] (1) Sample pretreatment

[0119] Weigh 5g of potatoes into a 50mL EP tube, crush them thoroughly, then add 10mL of deionized water, 10mL of dichloromethane and 2mL of dichloromethane in turn, mix and shake for 60min, then centrifuge at 8000r / min for 10min, take 9mL of the supernatant Then add 1mL acetonitrile; use 10mL methanol, 10mL acetonitrile and 10mL water to activate the C18 solid-phase microextraction column successively, and let it stand for 5min after the activation is completed; take the above-mentioned clear solution to the column for purification treatment, it is worth noting that, The flow rate cannot be faster than 1 drop / s, and the effluent is collected; finally, the purified sample is detected by liquid chromatography-mass spectrometry.

[0120] (2) Preparation of standard working solution

[0121] Use the tested potatoes that do not co...

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Abstract

The invention provides a method for determining residual quantity of glyphosate, glufosinate-ammonium and metabolite aminomethylphosphonic acid thereof in agricultural products. The method comprises the following steps: firstly, extracting and purifying glufosinate-ammonium, glyphosate and metabolite aminomethylphosphonic acid in a sample by adopting a solid-phase microextraction method, and then qualitatively and quantitatively detecting the glufosinate-ammonium, the glyphosate and the metabolite aminomethylphosphonic acid by adopting high performance liquid chromatography-tandem mass spectrometry and an internal standard method. According to the method disclosed by the invention, the lowest detection limits of glyphosate, glufosinate-ammonium and metabolite aminomethylphosphonic acid of the glyphosate, the glufosinate-ammonium and the metabolite aminomethylphosphonic acid are 0.03 mu g/kg, 0.29 mu g/kg and 0.39 mu g/kg. Compared with other detection methods, the method does not need a complex derivatization process, is high in detection efficiency, is simple and convenient, and is short in time consumption. By using the isotope internal standard, the interference caused by a series of reasons such as matrix effect can be avoided, and the quantitative result is more accurate. The method can also be used for simultaneously detecting three target objects including glyphosate, glufosinate-ammonium and aminomethylphosphonic acid in a complex sample, and is more efficient.

Description

technical field [0001] The invention relates to the technical field of pretreatment and detection of pesticide residues, in particular to a method for measuring residues of glyphosate, glufosinate-ammonium and their metabolite aminomethylphosphonic acid in agricultural products. Background technique [0002] Glyphosate, also known as Danon, and chemically named N-(phosphonic acid methyl) glycine, is a high-efficiency, low-toxicity, broad-spectrum herbicide. Glufosinate-ammonium is another broad-spectrum herbicide with excellent performance after glyphosate, and it is widely used in agriculture, forestry and other industries. Greenpeace reports show that glyphosate has effects on reproductive health and the nervous system, as well as carcinogenic effects. In order to prevent the accumulation of glyphosate in food, it is particularly important to strengthen the detection of glyphosate, its metabolite aminomethylphosphonic acid and glufosinate-ammonium residues in food. [00...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/30G01N30/32G01N30/34G01N30/72G01N30/86B01J20/281
Inventor 董军高梦月苏小路胡亦清肖康飞姚延兴易文晗陈洁李宝喜郑利
Owner WUHAN ACADEMY OF AGRI SCI
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